CN115368822A - Ceramizable high-temperature-resistant dimensional silicone rubber protective material and preparation method thereof - Google Patents
Ceramizable high-temperature-resistant dimensional silicone rubber protective material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ceramizable high-temperature-resistant dimensional silicone rubber protective material and a preparation method thereof, wherein the ceramizable high-temperature-resistant dimensional silicone rubber protective material comprises the following components in parts by weight: 100-110 parts of silicon rubber, 20-40 parts of fumed silica, 80-100 parts of functional filler, 20-30 parts of sintering aid, 10-30 parts of reinforcing fiber with the length of 0.5-3mm, 3-5 parts of silicone oil, 1-5 parts of silane coupling agent and 3-5 parts of vulcanizing agent, wherein the functional filler is a mixture of ceramic filler, flame-retardant filler and heat-conducting filler, the flame-retardant filler at least comprises flaky calcium silicate, and the material can be rapidly vitrified in a high-temperature combustion environment and has the advantages of low high temperature resistance and shrinkage rate and high strength.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a ceramizable high-temperature-resistant dimensional silicone rubber protective material and a preparation method thereof.
Background
With the rapid development of modern industry, when the fields of civil and military fire prevention and flame retardation face continuous hot oxygen erosion, higher performance requirements are provided for an outer layer thermal protection material, the silicon rubber is used as a novel thermal protection material due to excellent high temperature resistance and insulation performance after burning, the silicon rubber thermal protection material has certain flexibility at normal temperature, and a good joint part can respond to the rotation, stretching and compression of a lining material, so that the silicon rubber thermal protection material is a better protection substrate.
In order to improve the heat resistance of the silicone rubber, the silicone rubber is modified by related technologies, for example, chinese patent document CN 110128831A (application number: 201910353146.7) discloses a ceramic silicone rubber with excellent ceramic forming property and flame resistance, zirconium silicate, zirconium phosphate and the like are introduced into a substrate to realize that the ablation bending strength reaches 39.18MPa at 1000 ℃; chinese patent document CN 109021571A (application number: 2018 10598057.4) discloses a thermal response self-expansion ablation-resistant silicon rubber material, which can resist 15min ablation under flame by adding proper amount of aramid fiber, foaming agent, reinforcing agent and the like, and has the complete effect of a carbonized layer.
However, the material is foamed under a high-temperature environment to cause large internal porosity, the overall strength is rapidly reduced, and the problem that the material generates porcelain phase change reaction for improving the temperature resistance in actual use but has large size shrinkage after porcelain treatment is ignored.
Disclosure of Invention
In view of this, the present application provides a ceramizable high temperature resistant dimensional silicone rubber protective material and a preparation method thereof, and the material can be rapidly ceramizable in a high temperature combustion environment, and has the advantages of low high temperature resistance and shrinkage rate, and high strength.
In order to achieve the technical purpose, the following technical scheme is adopted in the application:
in a first aspect, the application provides a ceramizable high-temperature-resistant dimensional silicone rubber protective material, which comprises the following components in parts by weight: 100-110 parts of silicon rubber, 20-40 parts of fumed silica, 80-100 parts of functional filler, 20-30 parts of sintering aid, 10-30 parts of reinforcing fiber with the length of 0.5-3mm, 3-5 parts of silicone oil, 1-5 parts of silane coupling agent and 3-5 parts of vulcanizing agent, wherein the functional filler is a mixture of ceramic filler, flame-retardant filler and heat-conducting filler, and the flame-retardant filler at least comprises flaky calcium silicate.
Preferably, the reinforcing fiber comprises one or more of alumina whisker, carbon fiber whisker and quartz fiber.
Preferably, the sintering aid comprises one or more of zinc oxide, boron oxide, zinc borate and glass powder with an initial melting point of 450-550 ℃.
Preferably, the heat conducting filler comprises one or more of boron nitride, aluminum oxide and aluminum nitride.
Preferably, the fumed silica has a specific surface area of 80-320m 2 A hydrophobic fumed silica per gram.
Preferably, the silicone rubber comprises one or more of methyl vinyl silicone rubber and phenyl vinyl silicone rubber.
Preferably, the silicone oil comprises one or more of hydroxyl silicone oil, hydrogenated silicone oil and vinyl silicone oil.
In a second aspect, the application provides a preparation method of a ceramizable high-temperature-resistant dimensional silicone rubber protective material, which comprises the following steps:
s1, modifying a functional filler by using a silane coupling agent, and grinding to obtain a modified functional filler;
s2, mixing silicon rubber, fumed silica, a sintering aid, reinforcing fibers, a modified functional filler, silicone oil and a vulcanizing agent at room temperature, mixing the mixed rubber after mixing, and vulcanizing and forming to obtain the ceramizable high-temperature-resistant dimensional silicon rubber protective material.
In a third aspect, the application provides an application of the ceramizable high-temperature-resistant dimensional silicon rubber protective material as a flame-retardant, heat-insulating or insulating coating.
Preferably, the thickness of the coating is more than or equal to 2mm, and the application temperature is more than or equal to 800 ℃.
The beneficial effect of this application is as follows:
the silicone rubber protective material has the advantages of strong self-supporting property, high shape stability and rapid ceramization at high temperature, rapidly generates ceramization transformation to form a compact continuous composite ceramic phase on the surface of a base material in a continuous high-temperature static combustion environment, and has excellent dimensional stability before and after phase transformation conversion and no obvious shrinkage deformation;
in the face of a continuous high-temperature thermal oxidation environment, the silicon rubber material solves the technical difficulties that a special-shaped component with the thickness of more than 2mm is formed in one step and a vitrification reaction can be quickly responded after sintering, forms a flexible silicon rubber material with uniform components and stable ceramic phase, has better heat-proof, flame-retardant and insulating properties, has higher mechanical property and excellent dimensional stability after being completely formed and vitrified, has high strength and small shrinkage rate, and effectively insulates and supports an inner-layer matrix material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
For the problem of the great size shrink that appears after the quick response takes place ceramic phase transition reaction and the porcelain under balanced silicon rubber material high temperature, this application provides following technical scheme, but a high temperature resistant dimension shape silicon rubber protective material that can vitrify, including the component that the part by mass is as follows: 100-110 parts of silicon rubber, 20-40 parts of fumed silica, 80-100 parts of functional filler, 20-30 parts of sintering aid, 10-30 parts of reinforcing fiber with the length of 0.5-3mm, 3-5 parts of silicone oil, 1-5 parts of silane coupling agent and 3-5 parts of vulcanizing agent, wherein the functional filler is a mixture of ceramic filler, flame-retardant filler and heat-conducting filler, and the flame-retardant filler at least comprises flaky calcium silicate.
In the prior art, because the vitrification speed of the material is low, the thickness of a single-time coating is generally dozens of microns, multiple times of spraying are needed to achieve the required thickness to achieve the ideal thermal protection effect, but the problems of environment humidity, raw material proportion, non-uniform single-time spraying thickness and weak bonding force between sprayed layers can occur in each spraying process, meanwhile, the requirement on the particle size of the added filler is high due to the fact that the coating is too thin, the coating is not uniform, blockage caused by electrostatic force and the like can occur, the liquid phase viscosity of the application is low, the material has high thermal conductivity, the surface of the material can be quickly vitrified when the material meets high temperature, the material can quickly flow to form a compact ceramic body, the technical difficulties that a deformed component with the thickness of more than 2mm is formed in one step, the strength of the ceramic body after the material is sintered at the temperature of more than or equal to 800 ℃ and the ceramic body has excellent shape stability can be solved.
The ceramizable high-temperature-resistant dimensional silicone rubber protective material not only can be rapidly ceramized in a high-temperature combustion environment, but also has the advantages of high temperature resistance, low shrinkage and high strength, and the reasons and mechanisms are as follows: 1) The material has higher heat conductivity coefficient, and the surface of the material can be rapidly ceramic-treated to form a uniform multiphase ceramic layer when meeting high temperature; the flaky filler and the chopped reinforced fibers with higher proportion are mutually interpenetrated to form a complex cross-linked network to slow down the spread of hot air flow and resist high-temperature hot oxygen erosion in a short period; the molten liquid phase in the system can be filled along the cracked gap of the matrix to form a glass phase skeleton structure, and the density of the reinforced material forms a three-dimensional network protection structure; 2) CaSiO is introduced into the invention 3 At 850 ℃, alpha' -CaSiO can occur 3 →γ-CaSiO 3 The volume expansion of the crystal form is about 12 percent, and when the temperature is from 670 ℃ to cooling, the beta-CaSiO can occur 3 →γ-CaSiO 3 The crystal form of the silicon rubber has the volume expansion of about 10 percent after being converted, the volume shrinkage and the mass loss of the silicon rubber in a high-temperature combustion environment can be effectively counteracted, meanwhile, the obtained ceramic body has the self-supporting strength of 15MPa-18MPa, the size shrinkage rate after phase conversion is about 3 percent, and the ceramic body has better size stability so as to meet the practical use.
The reinforced fiber comprises one or more of alumina whisker, carbon fiber whisker and quartz fiber.
In order to reduce the porcelain forming temperature of the material, a sintering aid is added, wherein the sintering aid comprises one or more of zinc oxide, boron oxide, zinc borate and glass powder with an initial melting point of 450-550 ℃, and preferably, the sintering aid comprises a mixture of 450-DEG C low-melting-point glass powder, 550-DEG C low-melting-point glass powder, boron oxide and boron carbide in a mass ratio of 0.5.
The mixture of the functional material heat-conducting filler, the ceramic filler and the flame-retardant filler has the functions of improving the vitrification effect, improving the vitrification strength and accelerating the vitrification process, and the heat-conducting filler comprises one or more of boron nitride, aluminum oxide and aluminum nitride; the ceramic filler comprises one or more of kaolin, mica, bentonite and wollastonite, and the flame-retardant filler comprises at least one of magnesium hydroxide, aluminum hydroxide and calcium silicate.
The silane coupling agent is tetraethyl orthosilicate (TEOS), and specifically can be one or a mixture of more of silane coupling agents KH550, KH560, KH570, A171 and A172.
The fumed silica has a specific surface area of 80-320m 2 A hydrophobic fumed silica in a specific surface area of 200 to 300m 2 /g。
The silicon rubber comprises one or more of methyl vinyl silicon rubber and phenyl vinyl silicon rubber, preferably, the silicon rubber is phenyl vinyl silicon rubber, the content of phenyl is 5%, and the silicon rubber plays a role in connecting a main body in the material at normal temperature.
The silicone oil comprises one or more of hydroxyl silicone oil, hydrogenated silicone oil and vinyl silicone oil, and can play a role in improving the plasticity and the fluidity of the raw material in the material.
The vulcanizing agent is one of 2, 4-dichlorobenzoyl peroxide and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane.
Meanwhile, the application provides a preparation method of the ceramizable high-temperature-resistant dimensional silicone rubber protective material, which comprises the following steps:
s1, adding a functional filler into an ethanol water solution of TEOS (anhydrous ethanol: deionized water = 8);
s2, mixing silicon rubber, fumed silica, a sintering aid, reinforcing fibers, a modified functional filler, silicon oil and a vulcanizing agent at room temperature, putting the mixture into an open mill for uniformly mixing 3-5 times to obtain a rubber compound, and vulcanizing and molding the rubber compound at the roll temperature of the open mill of not higher than 80 ℃ to obtain the ceramizable high-temperature resistant dimensional silicon rubber protective material; the vulcanization conditions were: vulcanizing at 120-180 deg.C and 5-10MPa for 10-20min, and secondary vulcanizing at 180-220 deg.C for 1-3h.
The silicone rubber material has the heat insulation and high temperature resistance performances of high support performance and shape stability, can have good heat insulation and flame retardant performances and short-term high-temperature airflow scouring resistance in the face of a continuous high-temperature environment, can be rapidly ceramized in a short period, has high mechanical property and excellent dimensional stability after ablation, can be used as a flame-retardant, heat insulation or insulating coating without obvious shrinkage deformation, and has the thickness of more than or equal to 2mm and the application temperature of more than or equal to 800 ℃; at 800 ℃, the surface of the silicon rubber material can show a ceramic reaction phenomenon after static treatment for 5min at high temperature, a large amount of powder does not float out even though the material burns in the whole process, and meanwhile, flame can be extinguished in a short time after the material leaves a high-temperature environment, so that the silicon rubber material has a strong self-extinguishing effect; under 900 ℃, the surface of the ceramic shell appears after high-temperature static treatment for 3min, the bending strength reaches 5MPa, the pattern integrally appears in a completely ceramic state after ablation treatment for 15min, the bending strength reaches 15.8MPa, and the dimensional shrinkage rate is maintained to be less than 5%.
The present invention is further illustrated by the following specific examples.
Example 1
A ceramizable high-temperature-resistant dimensional silicone rubber protective material comprises the following components in parts by weight: 100 parts of silicon rubber, 35 parts of fumed silica, 90 parts of functional filler, 30 parts of sintering aid, 20 parts of quartz fiber with the length of 0.5mm, 3 parts of hydroxyl silicone oil, 3 parts of silane coupling agent and 2 parts of DBPH; the functional filler is a mixture of a ceramic filler, a flame-retardant filler and a heat-conducting filler, the ceramic filler is 30 parts of mica, the heat-conducting filler is a mixture of 10 parts of aluminum oxide and 20 parts of boron nitride, and the flame-retardant filler is a mixture of 15 parts of magnesium hydroxide and 15 parts of flaky calcium silicate; the sintering aid comprises the following components in percentage by mass of 0.5:1, 450 ℃, 550 ℃ melting point glass powder, B 2 O 3 、B 4 C, mixtures thereof.
The preparation method of the ceramizable high-temperature-resistant dimensional silicone rubber protective material comprises the following steps:
s1, adding 30g of functional filler into 100g of ethanol aqueous solution containing 3% TEOS (absolute ethanol: deionized water = 8;
s2, mixing silicon rubber, fumed silica, a sintering aid, reinforcing fibers, a modified functional filler, silicone oil and a vulcanizing agent according to a mass formula, putting the mixture into an open mill 3-5 times, mixing the mixture on a double-roll open mill, cleaning rollers before mixing, adjusting the distance between the rollers, and simultaneously adjusting the rotation speed ratio of the double rollers to be 1:1.2, taking down the rubber compound after uniformly mixing, filling the rubber compound into a clean die, putting the die into a flat vulcanizing machine, heating and vulcanizing to prepare a sheet with the thickness of 4mm, wherein the vulcanizing temperature is 170-180 ℃, the vulcanizing time is 10min, the pressure is 5-10MPa, and the vulcanizing time is 180-220 ℃, and the second-stage vulcanization is carried out for 4-6h to obtain the ceramizable high-temperature resistant dimensional silicon rubber protective material.
Example 2
A ceramizable high-temperature-resistant dimensional silicone rubber protective material is the same as in example 1 except that a heat-conducting filler is a mixture of 10 parts of aluminum oxide and 5 parts of aluminum nitride, and a flame-retardant filler is a mixture of 15 parts of aluminum hydroxide and 10 parts of flaky calcium silicate; the sintering aid comprises the following components in percentage by mass of 0.5:1, 450 ℃, 550 ℃ melting point glass powder, B 2 O 3 、B 4 C, a mixture thereof.
The preparation method is the same as in example 1.
Example 3
A ceramizable high-temperature-resistant dimensional silicone rubber protective material comprises the following components in parts by weight: 100 parts of silicon rubber, 30 parts of fumed silica, 85 parts of functional filler, 30 parts of sintering aid, 20 parts of alumina whisker with the length of 1mm, 3 parts of hydrogenated silicone oil, 3 parts of silane coupling agent and 2 parts of DBPH; the functional filler is a mixture of ceramic filler, flame-retardant filler and heat-conducting filler, the ceramic filler is 30 parts of kaolin, the heat-conducting filler is a mixture of 10 parts of alumina and 10 parts of aluminum nitride, and the heat-conducting filler isThe combustion filler is a mixture of 35 parts of flaky calcium silicate; the sintering aid comprises the following components in a mass ratio of 0.5:1, 450 ℃, 550 ℃ melting point glass powder, B 2 O 3 、B 4 C, mixtures thereof.
The preparation method is the same as in example 1.
Evaluation test
The performance of the ceramifiable high-temperature resistant dimensional silicone rubber protective material of the embodiment 1-2 of the present invention was tested by using commercial ceramifiable silicone rubber SR-0 as a blank control group, and the testing method was to test the mechanical properties after burning at 800 ℃ and record the ceramifiable time, and the results are shown in Table 1:
TABLE 1 comparison of the properties of the silicone rubber materials
At 800 ℃, the surface of the silicon rubber material can show a vitrification reaction phenomenon after static treatment at high temperature for 5min, although a large amount of powder does not fly out after the material burns in the whole process, and meanwhile, the flame of the material can be extinguished in a short time after the material leaves a high-temperature environment, so that the silicon rubber material has a strong self-extinguishing effect.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention.
Claims (10)
1. A ceramizable high-temperature-resistant dimensional silicone rubber protective material is characterized by comprising the following components in parts by weight: 100-110 parts of silicon rubber, 20-40 parts of fumed silica, 80-100 parts of functional filler, 20-30 parts of sintering aid, 10-30 parts of reinforcing fiber with the length of 0.5-3mm, 3-5 parts of silicone oil, 1-5 parts of silane coupling agent and 3-5 parts of vulcanizing agent, wherein the functional filler is a mixture of ceramic filler, flame-retardant filler and heat-conducting filler, and the flame-retardant filler at least comprises flaky calcium silicate.
2. The ceramifiable high-temperature resistant dimensional silicon rubber protective material as claimed in claim 1, wherein the reinforcing fibers comprise one or more of alumina whiskers, carbon fiber whiskers and quartz fibers.
3. The ceramifiable high-temperature-resistant dimensional silicone rubber protective material as claimed in claim 1, wherein the sintering aid comprises one or more of zinc oxide, boron oxide, zinc borate and glass powder with an initial melting point of 450-550 ℃.
4. The ceramifiable high-temperature resistant dimensional silicone rubber protective material as claimed in claim 1, wherein the heat conductive filler comprises one or more of boron nitride, aluminum oxide and aluminum nitride.
5. The ceramifiable high-temperature-resistant dimensional silicone rubber protective material as claimed in claim 1, wherein the fumed silica has a specific surface area of 80-320m 2 A hydrophobic fumed silica per gram.
6. The ceramifiable high-temperature resistant dimensional silicone rubber protective material as claimed in claim 1, wherein the silicone rubber comprises one or more of methyl vinyl silicone rubber and phenyl vinyl silicone rubber.
7. The ceramifiable high-temperature resistant dimensional silicone rubber protective material as claimed in claim 1, wherein the silicone oil comprises one or more of hydroxyl silicone oil, hydrogenated silicone oil and vinyl silicone oil.
8. The preparation method of the ceramifiable high-temperature resistant dimensional silicone rubber protective material as claimed in any one of claims 1 to 7, comprising the following steps:
s1, modifying the functional filler by using a silane coupling agent, and grinding to obtain a modified functional filler;
s2, mixing silicon rubber, fumed silica, a sintering aid, reinforcing fibers, a modified functional filler, silicone oil and a vulcanizing agent at room temperature, mixing the mixed rubber after mixing, and vulcanizing and forming to obtain the ceramizable high-temperature-resistant dimensional silicon rubber protective material.
9. Use of the ceramifiable high-temperature resistant dimensional silicone rubber protective material as defined in claims 1 to 7 as a flame retardant, heat insulating or insulating coating.
10. The use according to claim 9, wherein the coating has a thickness of 2mm or more and the temperature of the application is 800 ℃ or more.
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| CN115368822B (en) | 2023-06-06 |
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